CN113957563A - Low-melt-viscosity low-melting-point polyester fiber and preparation method and application thereof - Google Patents

Low-melt-viscosity low-melting-point polyester fiber and preparation method and application thereof Download PDF

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CN113957563A
CN113957563A CN202111504701.5A CN202111504701A CN113957563A CN 113957563 A CN113957563 A CN 113957563A CN 202111504701 A CN202111504701 A CN 202111504701A CN 113957563 A CN113957563 A CN 113957563A
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low
melting
point
polyester
fiber
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CN113957563B (en
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詹勇
孙毅
石宇
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Yangzhou Forewell Composite Materials Co ltd
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Yangzhou Forewell Composite Materials Co ltd
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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/68—Polyesters containing atoms other than carbon, hydrogen and oxygen
    • C08G63/682—Polyesters containing atoms other than carbon, hydrogen and oxygen containing halogens
    • C08G63/6824—Polyesters containing atoms other than carbon, hydrogen and oxygen containing halogens derived from polycarboxylic acids and polyhydroxy compounds
    • C08G63/6826—Dicarboxylic acids and dihydroxy compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/78—Preparation processes
    • C08G63/82—Preparation processes characterised by the catalyst used
    • C08G63/85—Germanium, tin, lead, arsenic, antimony, bismuth, titanium, zirconium, hafnium, vanadium, niobium, tantalum, or compounds thereof
    • C08G63/86—Germanium, antimony, or compounds thereof
    • C08G63/866—Antimony or compounds thereof
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/02—Cotton wool; Wadding
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4326—Condensation or reaction polymers
    • D04H1/435—Polyesters
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
    • D04H1/558—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving in combination with mechanical or physical treatments other than embossing
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres

Abstract

The invention relates to a low-melt-viscosity low-melting-point polyester fiber and a preparation method and application thereof, wherein the low-melt-viscosity low-melting-point polyester fiber has a sheath-core structure, the sheath layer is made of low-melting-point polyester (the molecular chain of the low-melting-viscosity low-melting-point polyester fiber consists of a terephthalic acid chain segment, a glycol chain segment, a 3-chloro-1, 2-butanediol chain segment and a diethylene glycol chain segment), and the core layer is made of conventional polyester; the preparation method comprises the following steps: respectively preparing conventional polyester and low-melting-point polyester, metering the conventional polyester and the low-melting-point polyester by a metering pump, and preparing the low-melting-point polyester fiber according to a sheath-core composite spinning process; the application is as follows: the low-melting-point polyester fiber with low melting viscosity and low melting point is mixed with other fibers according to a certain proportion, and then is made into the low-melting-point fiber flocculus through carding, web forming, hot drying and shaping treatment. The low-melt-viscosity low-melting-point polyester fiber has good melt fluidity and high glass transition temperature; the low-melting-point fiber flocculus prepared by the method has excellent compression performance and washing resistance.

Description

Low-melt-viscosity low-melting-point polyester fiber and preparation method and application thereof
Technical Field
The invention belongs to the technical field of low-melting-point polyester, and relates to low-melting-viscosity low-melting-point polyester fiber and a preparation method and application thereof.
Background
The low-melting-point polyester is obtained by modifying common polyester, has a lower melting point which is generally between 90 and 200 ℃, and retains partial characteristics of the common polyester due to the structural similarity with the chemical structure of the common polyester, and has good compatibility with the common polyester. The low-melting-point polyester can be melted at lower temperature, has stronger bonding performance, is mainly used for hot melt adhesive, and has the excellent performances of fast bonding, stable performance, good mechanical property, good elasticity, no toxicity, no pollution, low energy consumption and the like compared with other types of adhesives.
The production of the current low-melting-point polyester mainly takes isophthalic acid (IPA) and diethylene glycol (DEG) as modified components to be added into common PET polyester, the IPA is of an asymmetric structure, the addition of the IPA changes the symmetry of a molecular chain, destroys the original regular structure of the PET, and enables the arrangement of the chain to be loose, the motion capability to be increased and the melting point of the polyester to be reduced; the diethylene glycol has a longer main chain and also has an ether bond which enables a molecular chain to rotate easily, so that the flexibility of the molecular chain is greatly improved, and the melting point of polyester can be reduced.
At present, low-melting point polyester is widely applied to the non-woven fabric industry, in the non-woven fabric industry which is developed at a rapid speed at present, the thermal bonding method uses a fiber type adhesive processing method, so that the method is simple in processing, high in production speed, low in energy consumption and flexible in application, and the product does not contain any chemical reagent, so that the environment is not polluted, and the product is harmless to human bodies, so that the prior development is realized. The thermal bonding method is a reinforcing method which utilizes the thermoplasticity of a high molecular material, applies certain heat to a polymer fiber material to partially soften and melt the polymer fiber material, and bonds fibers together after cooling and solidification. For the polyester nonwoven industry, they require a polymer with a lower melting point than conventional polyesters and good compatibility with conventional polyesters as the thermally bondable fiber. According to the principle of "similar compatibility", the non-woven fabric using terylene as main fiber should be bonded by the same family polyester fiber, i.e. low melting point polyester.
However, the low-melting-point polyester has the problems of long melting range, high melt viscosity and the like at present, so that the low-melting-point polyester has poor fluidity when being melted and cannot be well dispersed in main fibers when being applied to the production of non-woven fabrics, thereby affecting the quality of subsequent products. However, this method reduces the glass transition temperature of the low-melting polyester while reducing the melt viscosity, which limits the range of applications of the low-melting polyester, and makes it possible to use it only at relatively low temperatures.
For non-woven fabrics (such as fiber flocculus), at a certain temperature, the sheath polymer with low melting point in the low-melting-point fiber is melted, so that the function of bonding and connecting fibers is realized in a fiber net, and the core polymer with high melting point and high strength is used for supporting the fiber net in bonding, so that the prepared flocculus has higher elastic recovery and bonding fastness. When the amount of the low-melting-point fibers to be bonded is constant, few brackets capable of performing bonding function are provided for the low-melting-point fibers with high melt viscosity, the bonding force between the main body fibers and the sheath-core composite fibers is weak, the bonding between the fibers of the flocculus is not firm, the bonding strength is poor, and the compression elastic rate is small. Therefore, the melt viscosity of the low-melting-point fiber is reduced, the fluidity of the low-melting-point fiber is improved, the bonding point can be effectively increased, and the bonding strength and the compression elastic modulus are improved.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a low-melt-viscosity low-melting-point polyester fiber and a preparation method and application thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a low-melt-viscosity low-melting-point polyester fiber has a sheath-core structure, wherein the sheath layer is made of low-melt-point polyester, and the core layer is made of conventional polyester (i.e. unmodified ethylene terephthalate);
the low-melting-point polyester is modified polyester, and a molecular chain of the modified polyester consists of a terephthalic acid chain segment, an ethylene glycol chain segment, a 3-chloro-1, 2-butanediol chain segment and a diethylene glycol chain segment; the molecular chain of the conventional polyester consists of a terephthalic acid chain segment and an ethylene glycol chain segment;
the glass transition temperature of the low-melting-point polyester is 68-72 ℃, the melting point is 100-130 ℃, the viscous flow activation energy is 21.6-30.3 kJ/mol, the viscous flow activation energy of the conventional polyester is 79.2kJ/mol, and the viscous flow activation energy of the low-melting-point polyester in the prior art is 34.7-56.3 kJ/mol. Viscous flow activation energy (E η) is a measure of the energy barrier that a high polymer melt needs to overcome to produce viscous flow and can be used to evaluate melt viscosity. When the molecular chain has good flexibility, the potential barrier for rotation in the chain is low, and the flow unit chain segment is short. The viscous flow activation energy of the low-melting-point polyester is much lower than that of the common low-melting-point copolyester (34.7-56.3 kJ/mol), and mainly 3-chloro-1, 2-butanediol contains branched chains, the length of the branched chains is not entangled, the interaction force among branched molecules is small, and the potential barrier of in-chain rotation is low, so that the energy required by the movement of molecular chain segments is relatively small, the viscous flow activation energy is low, and relatively large relative displacement among molecules can be generated at the same temperature.
As a preferred technical scheme:
the low-melt-viscosity and low-melting-point polyester fiber has the advantages that the molar ratio of the terephthalic acid chain segment, the ethylene glycol chain segment, the 3-chloro-1, 2-butanediol chain segment and the diethylene glycol chain segment in the molecular chain of the modified polyester is 1: 0.53-0.62: 0.29-0.34: 0.09-0.13; the molar ratio of the terephthalic acid chain segment to the ethylene glycol chain segment in the molecular chain of the conventional polyester is 1:1. In the polyester synthesis process, the boiling point of ethylene glycol is about 199 ℃, the boiling point of 3-chloro-1, 2-butanediol is about 220 ℃ which is far higher than the boiling point of ethylene glycol, and in the polycondensation process, when vacuum is pumped, ethylene glycol is mainly pumped out, and 3-chloro-1, 2-butanediol is rarely pumped out and basically consistent with the feeding amount; the boiling point of diethylene glycol is higher, around 245 ℃, and about 1.0 mol% of diethylene glycol of PET is formed in the polyester synthesis, so that the amount of diethylene glycol in the copolyester is increased.
The low-melt-viscosity and low-melting-point polyester fiber has the filament number of 4-5 dtex, the breaking strength of more than or equal to 3.8cN/dtex, the elongation at break of 50-60%, the number of crimps of 8-12/25 mm and the fiber length of 51 mm.
The polyester fiber with low melting viscosity and low melting point has a sheath-core ratio of 45-55: 55-45.
The low-melting-viscosity low-melting-point polyester fiber has a number average molecular weight of 20000 to 25000g/mol and a molecular weight distribution D of 2.2 to 3.0.
The present invention also provides a method for preparing the low-melt-viscosity low-melting-point polyester fiber as described in any one of the above, comprising the steps of:
(1) preparing conventional polyester;
preparing terephthalic acid, ethylene glycol, a catalyst and a stabilizer into slurry, carrying out esterification reaction, and after the esterification reaction is finished, sequentially carrying out polycondensation reaction in a low vacuum stage and polycondensation reaction in a high vacuum stage under the condition of negative pressure to prepare conventional polyester; the pressure of the polycondensation reaction in the low vacuum stage is 5000-500 Pa, and the pressure of the polycondensation reaction in the high vacuum stage is less than 100 Pa;
(2) preparing low-melting-point polyester;
preparing terephthalic acid, ethylene glycol, 3-chloro-1, 2-butanediol, diethylene glycol, a catalyst and a stabilizer into slurry, and then carrying out esterification reaction to obtain an esterification product; after the esterification reaction is finished, heating, stirring and mixing, and sequentially carrying out the polycondensation reaction in a low vacuum stage and the polycondensation reaction in a high vacuum stage under the condition of negative pressure to prepare modified polyester, namely low-melting-point polyester; the pressure of the polycondensation reaction in the low vacuum stage is 5000-500 Pa, and the pressure of the polycondensation reaction in the high vacuum stage is less than 100 Pa;
(3) preparing low-melting-viscosity low-melting-point polyester fibers;
and (2) accurately metering the conventional polyester prepared in the step (1) and the low-melting-point polyester prepared in the step (2) by a metering pump, and then spinning, cooling, bundling, stretching, curling, cutting (the length after cutting is 51mm), drying and packaging according to a skin-core composite spinning process to obtain the low-melting-point polyester fiber.
As a preferred technical scheme:
in the method, the temperature of the esterification reaction in the step (1) is 240-260 ℃, the end point of the esterification reaction is that the distilled amount of water reaches more than 95% of a theoretical value, the temperature of the polycondensation reaction is 275-280 ℃, and the reaction time is 60-90 minutes;
in the step (2), the temperature of the esterification reaction is 220-260 ℃, the end point of the esterification reaction is that the distilled amount of water reaches more than 95% of a theoretical value, the temperature of the polycondensation reaction is 265-275 ℃, and the reaction time is 50-90 minutes;
the technological parameters in the step (3) are as follows: the spinning temperature is 270-275 ℃, and the spinning speed is 1000-1200 m/min; the air temperature of the circular blowing air is 20-23 ℃, and the air speed of the circular blowing air is 7.0-8.0 m/s; the drawing multiple is 2.5-3.3 times, and the temperature of a drawing oil bath groove is 75-80 ℃; the drying temperature is 70-75 ℃.
The method comprises the following steps of (1) enabling the molar ratio of terephthalic acid to ethylene glycol to be 1: 1.3-1.6;
in the step (2), the molar ratio of the terephthalic acid to the ethylene glycol to the 3-chloro-1, 2-butanediol to the diethylene glycol is 1: 1.1-1.3: 0.30-0.35: 0.08-0.12;
the catalyst in the step (1) and the step (2) is antimony trioxide, ethylene glycol antimony or antimony acetate, the stabilizer is triphenyl phosphate, trimethyl phosphate or trimethyl phosphite, the adding amount of the catalyst is 0.018 to 0.020 percent of the mass of the terephthalic acid, and the adding amount of the stabilizer is 0.01 to 0.03 percent of the mass of the terephthalic acid.
The invention also provides the application of the low-melting-viscosity low-melting-point polyester fiber, the low-melting-viscosity low-melting-point polyester fiber is mixed with other fibers according to a certain proportion, and the mixture is carded into a net, thermally dried and shaped to prepare the low-melting-point fiber flocculus;
other fibers are PET fibers and three-dimensional crimped hollow polyester (specification 6.6dtex is multiplied by 51mm, Yangzhou Fuweil composite Co., Ltd.);
the surface density of the low-melting-point fiber flocculus is 200g/m2(ii) a The compression elasticity of the low-melting-point fiber flocculus is 93.7-95.1% (the compression performance of the flocculus reflects the performance of the flocculus after the flocculus is subjected to an acting force vertical to the plane of the flocculus, and is one of the important performances of the flocculus, particularly for medium-thickness flocculus, the deformation recovery capability after a heavy object is borne is mainly reflected, and the filling power, the compression elasticity and the compression ratio are usually used for measuring the compression elasticity of the flocculus, namely the deformation resistance capability of the flocculus in the compression process, and the bonding strength of the low-melting-point fiber is reflected, the compression elasticity shows that the bonding strength of the low-melting-point fiber is higher, the compression elasticity of the low-melting-point fiber flocculus in the prior art is 78.3-89.1%), the warp fracture strength is 12.72-13.21N, and the weft fracture strength is 8.17-8.36N (the bonding strength can be represented by the warp and weft fracture strengths); the strength reduction rates of the low-melting-point fiber flocculus in the warp direction and the weft direction before and after washing are respectively 10.3-12.9% and 13.1-15.7% according to the FZ/T64003-1993 test, wherein the breaking strength of the low-melting-point fiber flocculus in the prior art is 10.33-10.82N (in the warp direction) and 6.86-7.01N (in the weft direction), and the strength reduction rates before and after washing are 20.2-22.7% (in the warp direction and 23.1-25.5% (in the weft direction) according to the FZ/T64003-1993 test.
As a preferred technical scheme:
the application is characterized in that the mass ratio of the low-melting-viscosity low-melting-point polyester fiber to the PET fiber to the three-dimensional curled hollow polyester fiber is 15:60: 25;
the length of the PET fiber is 51mm, and the fineness is 3.3 dtex; the length of the three-dimensional curled hollow polyester is 51mm, and the fineness is 6.6 dtex.
The invention mechanism is as follows:
the 3-chloro-1, 2-butanediol is used for replacing isophthalic acid as a third component to prepare the low-melting-point polyester with low melting viscosity, the branched chain structure is an important factor influencing the melt viscosity of the high polymer, the 3-chloro-1, 2-butanediol contains branched chains, the branched chain length is not entangled, the interaction force between branched molecules is small, and the reduction of the melt viscosity of the high polymer is facilitated. The introduction of 3-chlorine-1, 2-butanediol increases the free volume of a macromolecular chain, so that the viscosity of the prepared low-melting-point polyester is reduced during melting, the dispersibility is better, the contribution of the glass transition temperature of the modified polyester to rigid terephthalic acid is large, the main chain length of the 3-chlorine-1, 2-butanediol is the same as that of ethylene glycol, the length of a branched chain is not large, and the phenomenon of low glass transition temperature after the introduction of a long chain segment cannot be generated.
The existence of the branched chain can increase the steric hindrance of a molecular chain, so that water molecules are difficult to approach ester groups, the hydrolysis reaction of the ester groups is hindered, and the hydrolysis resistance of the low-melting-point polyester is greatly improved; meanwhile, the-Cl is a hydrophobic group, and the-Cl in the 3-chloro-1, 2-butanediol is beneficial to further improving the hydrolysis resistance.
The principle that the low-melting-point polyester can be bonded with the main body fiber is that the low-melting-point polyester can generate van der Waals force and physical adsorption such as hydrogen bond between the low-melting-point polyester and the main body fiber, the bonding property is good, but with the continuous improvement of living standard of people, the requirement on the bonding strength of the low-melting-point polyester is higher and higher. The introduction of 3-chloro-1, 2-butanediol can not only reduce the melt viscosity of the low-melting polyester, but also improve the bonding strength of the low-melting polyester, because the branched chain of the 3-chloro-1, 2-butanediol is provided with a chlorine atom, and after the hydrogen atom in the 3-chloro-1, 2-butanediol is bonded with a carbon atom, under the action of the chlorine atom with stronger electronegativity, the C-H common electron pair is deflected to one side of the carbon atom, and the hydrogen atom nucleus with positive charge is almost exposed outside. During bonding, the low-melting-point polyester has sufficient contact with the main fiber under the action of the chlorine atom with stronger electronegativity; and the hydrogen atoms showing positive charges in the 3-chloro-1, 2-butanediol can generate induced orientation on chlorine atoms or oxygen atoms (including chlorine atoms or oxygen atoms on other chain segments in the same macromolecular chain and chlorine atoms or oxygen atoms on other macromolecular chains) with stronger electronegativity of other chain segments, so that the molecular chains are closer to each other under the action of an induced force, hydrogen bonds are more easily generated, and the bonding strength is improved.
Has the advantages that:
(1) the low-melt-viscosity low-melting-point polyester fiber has good melt fluidity, high glass transition temperature and good application prospect;
(2) the preparation method of the low-melting-viscosity low-melting-point polyester fiber is simple and feasible, and the low-melting-viscosity low-melting-point polyester fiber can be prepared only by adopting 3-chloro-1, 2-butanediol to replace isophthalic acid as a third component;
(3) the low-melting-point polyester fiber with low melting viscosity is used for preparing the low-melting-point fiber flocculus, and the prepared low-melting-point fiber flocculus has excellent compression performance and washing resistance.
Detailed Description
The invention will be further illustrated with reference to specific embodiments. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
The main performance test method in the invention is as follows:
viscous flow activation energy: the test method is described in the literature "rheological Properties of Low melting copolyesters [ J ]. Industrial textiles, 2007(05):17-19 ].
Compression modulus of elasticity: the compression elasticity was determined according to the method described in Standard FZ/T64003-1993 "SprayIng batts".
Water washing resistance: reference is made to the test procedure for water resistance in the Standard FZ/T64003-1993 "sprayed Cotton batting". The test of the breaking strength in the warp direction and the weft direction was carried out in accordance with the standard FZ/T60005-1991 "determination of breaking strength and elongation at break of nonwoven fabric".
Example 1
A preparation method of low-melt viscosity and low-melting point polyester fiber comprises the following specific steps:
(1) preparing conventional polyester;
preparing terephthalic acid, ethylene glycol, a catalyst (antimony trioxide) and a stabilizer (triphenyl phosphate) into slurry, then carrying out esterification reaction, and after the esterification reaction is finished, sequentially carrying out polycondensation reaction in a low vacuum stage (the pressure is 5000Pa) and polycondensation reaction in a high vacuum stage (the pressure is 95Pa) under the condition of negative pressure to prepare conventional polyester; wherein the molar ratio of the terephthalic acid to the ethylene glycol is 1:1.3, the adding amount of the catalyst is 0.018 percent of the mass of the terephthalic acid, and the adding amount of the stabilizer is 0.01 percent of the mass of the terephthalic acid; the temperature of the esterification reaction was 240 ℃, the end point of the esterification reaction was 95% of the theoretical value of the distilled amount of water, the temperature of the polycondensation reaction was 275 ℃, and the reaction time was 90 minutes (wherein the reaction time in the low vacuum stage was 65 minutes);
(2) preparing low-melting-point polyester;
preparing terephthalic acid, ethylene glycol, 3-chloro-1, 2-butanediol, diethylene glycol, a catalyst (antimony trioxide) and a stabilizer (triphenyl phosphate) into slurry, and then carrying out esterification reaction to obtain an esterification product; after the esterification reaction is finished, heating, stirring and mixing, and sequentially carrying out polycondensation reaction in a low vacuum stage (with the pressure of 5000Pa) and polycondensation reaction in a high vacuum stage (with the pressure of 95Pa) under the condition of negative pressure to prepare modified polyester, namely low-melting-point polyester; wherein the molar ratio of the terephthalic acid to the ethylene glycol to the 3-chloro-1, 2-butanediol to the diethylene glycol is 1:1.1:0.30:0.08, the adding amount of the catalyst is 0.018 percent of the mass of the terephthalic acid, and the adding amount of the stabilizer is 0.01 percent of the mass of the terephthalic acid; the temperature of the esterification reaction was 220 ℃, the end point of the esterification reaction was 95% of the theoretical value of the distilled amount of water, the temperature of the polycondensation reaction was 265 ℃, and the reaction time was 90 minutes (wherein the reaction time in the low vacuum stage was 45 minutes);
the number average molecular weight of the prepared low-melting-point polyester is 20000g/mol, the molecular weight distribution D is 2.7, the glass transition temperature is 69 ℃, the melting point is 118 ℃, and the viscous flow activation energy is 25.8 kJ/mol;
(3) preparing low-melting-viscosity low-melting-point polyester fibers;
metering the conventional polyester prepared in the step (1) and the low-melting-point polyester prepared in the step (2) by a metering pump, and then spinning, cooling, bundling, stretching, curling, cutting, drying and packaging according to a skin-core composite spinning process to obtain low-melting-point polyester fibers; wherein the technological parameters are as follows: the spinning temperature is 270 ℃, and the spinning speed is 1000 m/min; the air temperature of the circular blowing air is 20 ℃, and the air speed of the circular blowing air is 7.0 m/s; the drawing multiple is 2.5 times, and the temperature of a drawing oil bath groove is 75 ℃; the drying temperature was 70 ℃.
The finally prepared low-melt-viscosity low-melting-point polyester fiber has a sheath-core structure, the sheath-core ratio is 45:55, the sheath layer is made of low-melting-point polyester, and the core layer is made of conventional polyester; the low melt viscosity and low melting point polyester fiber has a filament number of 4dtex, a breaking strength of 3.8cN/dtex, an elongation at break of 50%, a number of crimps of 8/25 mm, and a fiber length of 51 mm.
Example 2
A preparation method of low-melt viscosity and low-melting point polyester fiber comprises the following specific steps:
(1) preparing conventional polyester;
preparing terephthalic acid, ethylene glycol, a catalyst (antimony trioxide) and a stabilizer (triphenyl phosphate) into slurry, then carrying out esterification reaction, and after the esterification reaction is finished, sequentially carrying out polycondensation reaction in a low vacuum stage (the pressure is 4500Pa) and polycondensation reaction in a high vacuum stage (the pressure is 90Pa) under the condition of negative pressure to prepare conventional polyester; wherein the molar ratio of the terephthalic acid to the ethylene glycol is 1:1.3, the adding amount of the catalyst is 0.018 percent of the mass of the terephthalic acid, and the adding amount of the stabilizer is 0.01 percent of the mass of the terephthalic acid; the temperature of the esterification reaction was 240 ℃, the end point of the esterification reaction was 96% of the theoretical value of the distilled amount of water, the temperature of the polycondensation reaction was 275 ℃, and the reaction time was 90 minutes (wherein the reaction time in the low vacuum stage was 70 minutes);
(2) preparing low-melting-point polyester;
preparing terephthalic acid, ethylene glycol, 3-chloro-1, 2-butanediol, diethylene glycol, a catalyst (antimony trioxide) and a stabilizer (triphenyl phosphate) into slurry, and then carrying out esterification reaction to obtain an esterification product; after the esterification reaction is finished, heating, stirring and mixing, and sequentially carrying out polycondensation reaction in a low vacuum stage (pressure is 4500Pa) and polycondensation reaction in a high vacuum stage (pressure is 50Pa) under the condition of negative pressure to prepare modified polyester, namely low-melting-point polyester; wherein the molar ratio of the terephthalic acid to the ethylene glycol to the 3-chloro-1, 2-butanediol to the diethylene glycol is 1:1.1:0.30:0.12, the adding amount of the catalyst is 0.018 percent of the mass of the terephthalic acid, and the adding amount of the stabilizer is 0.01 percent of the mass of the terephthalic acid; the temperature of the esterification reaction was 224 ℃, the end point of the esterification reaction was 96% of the theoretical value of the distilled amount of water, the temperature of the polycondensation reaction was 265 ℃, and the reaction time was 90 minutes (wherein the reaction time in the low vacuum stage was 65 minutes);
the number average molecular weight of the prepared low-melting-point polyester is 25000g/mol, the molecular weight distribution D is 2.6, the glass transition temperature is 70 ℃, the melting point is 120 ℃, and the viscous flow activation energy is 28.7 kJ/mol;
(3) preparing low-melting-viscosity low-melting-point polyester fibers;
metering the conventional polyester prepared in the step (1) and the low-melting-point polyester prepared in the step (2) by a metering pump, and then spinning, cooling, bundling, stretching, curling, cutting, drying and packaging according to a skin-core composite spinning process to obtain low-melting-point polyester fibers; wherein the technological parameters are as follows: the spinning temperature is 270 ℃, and the spinning speed is 1000 m/min; the air temperature of the circular blowing air is 20 ℃, and the air speed of the circular blowing air is 7.2 m/s; the drawing multiple is 2.8 times, and the temperature of a drawing oil bath groove is 75 ℃; the drying temperature was 70 ℃.
The finally prepared low-melt-viscosity low-melting-point polyester fiber has a sheath-core structure, the sheath-core ratio is 50:50, the sheath layer is made of low-melting-point polyester, and the core layer is made of conventional polyester; the low melt viscosity and low melting point polyester fiber has a filament fineness of 5dtex, a breaking strength of 3.9cN/dtex, an elongation at break of 54%, a crimp number of 12/25 mm, and a fiber length of 51 mm.
Example 3
A preparation method of low-melt viscosity and low-melting point polyester fiber comprises the following specific steps:
(1) preparing conventional polyester;
preparing terephthalic acid, ethylene glycol, a catalyst (ethylene glycol antimony) and a stabilizer (trimethyl phosphate) into slurry, then carrying out esterification reaction, and after the esterification reaction is finished, sequentially carrying out polycondensation reaction in a low vacuum stage (the pressure is 4500Pa) and polycondensation reaction in a high vacuum stage (the pressure is 90Pa) under the condition of negative pressure to prepare conventional polyester; wherein the molar ratio of the terephthalic acid to the ethylene glycol is 1:1.4, the adding amount of the catalyst is 0.018 percent of the mass of the terephthalic acid, and the adding amount of the stabilizer is 0.02 percent of the mass of the terephthalic acid; the temperature of the esterification reaction was 250 ℃, the end point of the esterification reaction was 98% of the theoretical value of the distilled amount of water, the temperature of the polycondensation reaction was 275 ℃, and the reaction time was 86 minutes (wherein the reaction time in the low vacuum stage was 68 minutes);
(2) preparing low-melting-point polyester;
preparing terephthalic acid, ethylene glycol, 3-chloro-1, 2-butanediol, diethylene glycol, a catalyst (ethylene glycol antimony) and a stabilizer (trimethyl phosphate) into slurry, and then carrying out esterification reaction to obtain an esterification product; after the esterification reaction is finished, heating, stirring and mixing, and sequentially carrying out polycondensation reaction in a low vacuum stage (pressure is 4500Pa) and polycondensation reaction in a high vacuum stage (pressure is 34Pa) under the condition of negative pressure to prepare modified polyester, namely low-melting-point polyester; wherein the molar ratio of the terephthalic acid to the ethylene glycol to the 3-chloro-1, 2-butanediol to the diethylene glycol is 1:1.3:0.30:0.08, the adding amount of the catalyst is 0.018 percent of the mass of the terephthalic acid, and the adding amount of the stabilizer is 0.02 percent of the mass of the terephthalic acid; the temperature of the esterification reaction was 235 ℃, the end point of the esterification reaction was 98% of the theoretical value of the distilled amount of water, the temperature of the polycondensation reaction was 268 ℃, and the reaction time was 85 minutes (wherein the reaction time in the low vacuum stage was 55 minutes);
the number average molecular weight of the prepared low-melting-point polyester is 23400g/mol, the molecular weight distribution D is 2.9, the glass transition temperature is 68 ℃, the melting point is 116 ℃, and the viscous flow activation energy is 29.6 kJ/mol;
(3) preparing low-melting-viscosity low-melting-point polyester fibers;
metering the conventional polyester prepared in the step (1) and the low-melting-point polyester prepared in the step (2) by a metering pump, and then spinning, cooling, bundling, stretching, curling, cutting, drying and packaging according to a skin-core composite spinning process to obtain low-melting-point polyester fibers; wherein the technological parameters are as follows: the spinning temperature is 272 ℃, and the spinning speed is 1040 m/min; the air temperature of the circular blowing air is 22 ℃, and the air speed of the circular blowing air is 7.5 m/s; the drawing multiple is 3.0 times, and the temperature of a drawing oil bath groove is 78 ℃; the drying temperature was 72 ℃.
The finally prepared low-melt-viscosity low-melting-point polyester fiber has a sheath-core structure, the sheath-core ratio is 50:50, the sheath layer is made of low-melting-point polyester, and the core layer is made of conventional polyester; the low melt viscosity and low melting point polyester fiber has a single filament fineness of 4.5dtex, a breaking strength of 4.0cN/dtex, an elongation at break of 60%, a crimp number of 11/25 mm, and a fiber length of 51 mm.
Example 4
A preparation method of low-melt viscosity and low-melting point polyester fiber comprises the following specific steps:
(1) preparing conventional polyester;
preparing terephthalic acid, ethylene glycol, a catalyst (ethylene glycol antimony) and a stabilizer (trimethyl phosphate) into slurry, then carrying out esterification reaction, and after the esterification reaction is finished, sequentially carrying out polycondensation reaction in a low vacuum stage (pressure of 3000Pa) and polycondensation reaction in a high vacuum stage (pressure of 88Pa) under the condition of negative pressure to prepare conventional polyester; wherein the molar ratio of the terephthalic acid to the ethylene glycol is 1:1.5, the adding amount of the catalyst is 0.018 percent of the mass of the terephthalic acid, and the adding amount of the stabilizer is 0.03 percent of the mass of the terephthalic acid; the temperature of the esterification reaction was 255 ℃, the end point of the esterification reaction was 98% of the theoretical value of the distilled amount of water, the temperature of the polycondensation reaction was 278 ℃, and the reaction time was 80 minutes (wherein the reaction time in the low vacuum stage was 72 minutes);
(2) preparing low-melting-point polyester;
preparing terephthalic acid, ethylene glycol, 3-chloro-1, 2-butanediol, diethylene glycol, a catalyst (ethylene glycol antimony) and a stabilizer (trimethyl phosphate) into slurry, and then carrying out esterification reaction to obtain an esterification product; after the esterification reaction is finished, heating, stirring and mixing, and sequentially carrying out polycondensation reaction in a low vacuum stage (pressure is 3000Pa) and polycondensation reaction in a high vacuum stage (pressure is 27Pa) under the condition of negative pressure to prepare modified polyester, namely low-melting-point polyester; wherein the molar ratio of the terephthalic acid to the ethylene glycol to the 3-chloro-1, 2-butanediol to the diethylene glycol is 1:1.3:0.35:0.12, the adding amount of the catalyst is 0.018 percent of the mass of the terephthalic acid, and the adding amount of the stabilizer is 0.03 percent of the mass of the terephthalic acid; the temperature of the esterification reaction was 240 ℃, the end point of the esterification reaction was 98% of the theoretical value of the distilled amount of water, the temperature of the polycondensation reaction was 270 ℃, and the reaction time was 73 minutes (wherein the reaction time in the low vacuum stage was 50 minutes);
the number average molecular weight of the prepared low-melting-point polyester is 22600g/mol, the molecular weight distribution D is 3.0, the glass transition temperature is 69 ℃, the melting point is 110 ℃, and the viscous flow activation energy is 22.5 kJ/mol;
(3) preparing low-melting-viscosity low-melting-point polyester fibers;
metering the conventional polyester prepared in the step (1) and the low-melting-point polyester prepared in the step (2) by a metering pump, and then spinning, cooling, bundling, stretching, curling, cutting, drying and packaging according to a skin-core composite spinning process to obtain low-melting-point polyester fibers; wherein the technological parameters are as follows: the spinning temperature is 275 ℃, and the spinning speed is 1080 m/min; the air temperature of the circular blowing air is 23 ℃, and the air speed of the circular blowing air is 7.5 m/s; the drawing multiple is 3.2 times, and the temperature of a drawing oil bath groove is 80 ℃; the drying temperature was 75 ℃.
The finally prepared low-melt-viscosity low-melting-point polyester fiber has a sheath-core structure, the sheath-core ratio is 50:50, the sheath layer is made of low-melting-point polyester, and the core layer is made of conventional polyester; the low melt viscosity and low melting point polyester fiber has a single filament fineness of 4.5dtex, a breaking strength of 4.0cN/dtex, an elongation at break of 55%, a crimp number of 12/25 mm, and a fiber length of 51 mm.
Example 5
A preparation method of low-melt viscosity and low-melting point polyester fiber comprises the following specific steps:
(1) preparing conventional polyester;
preparing terephthalic acid, ethylene glycol, a catalyst (antimony acetate) and a stabilizer (trimethyl phosphite) into slurry, then carrying out esterification reaction, and after the esterification reaction is finished, sequentially carrying out polycondensation reaction in a low vacuum stage (the pressure is 2500Pa) and polycondensation reaction in a high vacuum stage (the pressure is 85Pa) under the condition of negative pressure to prepare conventional polyester; wherein the molar ratio of the terephthalic acid to the ethylene glycol is 1:1.6, the adding amount of the catalyst is 0.020% of the mass of the terephthalic acid, and the adding amount of the stabilizer is 0.03% of the mass of the terephthalic acid; the temperature of the esterification reaction was 260 ℃, the end point of the esterification reaction was 98% of the theoretical value of the distilled amount of water, the temperature of the polycondensation reaction was 280 ℃, and the reaction time was 60 minutes (wherein the reaction time in the low vacuum stage was 55 minutes);
(2) preparing low-melting-point polyester;
preparing terephthalic acid, ethylene glycol, 3-chloro-1, 2-butanediol, diethylene glycol, a catalyst (antimony acetate) and a stabilizer (trimethyl phosphite) into slurry, and then carrying out esterification reaction to obtain an esterification product; after the esterification reaction is finished, heating, stirring and mixing, and sequentially carrying out polycondensation reaction in a low vacuum stage (the pressure is 2500Pa) and polycondensation reaction in a high vacuum stage (the pressure is 65Pa) under the condition of negative pressure to prepare modified polyester, namely low-melting-point polyester; wherein the molar ratio of the terephthalic acid to the ethylene glycol to the 3-chloro-1, 2-butanediol to the diethylene glycol is 1:1.3:0.35:0.10, the addition amount of the catalyst is 0.020% of the mass of the terephthalic acid, and the addition amount of the stabilizer is 0.03% of the mass of the terephthalic acid; the temperature of the esterification reaction was 260 ℃, the end point of the esterification reaction was that the distilled amount of water reached 98% of the theoretical value, the temperature of the polycondensation reaction was 275 ℃, and the reaction time was 60 minutes (wherein the reaction time in the low vacuum stage was 45 minutes);
the number average molecular weight of the prepared low-melting-point polyester is 21800g/mol, the molecular weight distribution D is 2.2, the glass transition temperature is 69 ℃, the melting point is 100 ℃, and the viscous flow activation energy is 21.6 kJ/mol;
(3) preparing low-melting-viscosity low-melting-point polyester fibers;
metering the conventional polyester prepared in the step (1) and the low-melting-point polyester prepared in the step (2) by a metering pump, and then spinning, cooling, bundling, stretching, curling, cutting, drying and packaging according to a skin-core composite spinning process to obtain low-melting-point polyester fibers; wherein the technological parameters are as follows: the spinning temperature is 275 ℃, and the spinning speed is 1100 m/min; the air temperature of the circular blowing air is 23 ℃, and the air speed of the circular blowing air is 7.5 m/s; the drawing multiple is 3.2 times, and the temperature of a drawing oil bath groove is 80 ℃; the drying temperature was 75 ℃.
The finally prepared low-melt-viscosity low-melting-point polyester fiber has a sheath-core structure, the sheath-core ratio is 50:50, the sheath layer is made of low-melting-point polyester, and the core layer is made of conventional polyester; the low melt viscosity and low melting point polyester fiber has a single filament fineness of 4dtex, a breaking strength of 3.8cN/dtex, an elongation at break of 52%, a crimp number of 10/25 mm, and a fiber length of 51 mm.
Example 6
A preparation method of low-melt viscosity and low-melting point polyester fiber comprises the following specific steps:
(1) preparing conventional polyester;
preparing terephthalic acid, ethylene glycol, a catalyst (antimony acetate) and a stabilizer (trimethyl phosphite) into slurry, then carrying out esterification reaction, and after the esterification reaction is finished, sequentially carrying out polycondensation reaction in a low vacuum stage (the pressure is 500Pa) and polycondensation reaction in a high vacuum stage (the pressure is 85Pa) under the condition of negative pressure to prepare conventional polyester; wherein the molar ratio of the terephthalic acid to the ethylene glycol is 1:1.6, the adding amount of the catalyst is 0.020% of the mass of the terephthalic acid, and the adding amount of the stabilizer is 0.03% of the mass of the terephthalic acid; the temperature of the esterification reaction was 260 ℃, the end point of the esterification reaction was 98% of the theoretical value of the distilled amount of water, the temperature of the polycondensation reaction was 280 ℃, and the reaction time was 60 minutes (wherein the reaction time in the low vacuum stage was 54 minutes);
(2) preparing low-melting-point polyester;
preparing terephthalic acid, ethylene glycol, 3-chloro-1, 2-butanediol, diethylene glycol, a catalyst (antimony acetate) and a stabilizer (trimethyl phosphite) into slurry, and then carrying out esterification reaction to obtain an esterification product; after the esterification reaction is finished, heating, stirring and mixing, and sequentially carrying out polycondensation reaction in a low vacuum stage (the pressure is 500Pa) and polycondensation reaction in a high vacuum stage (the pressure is 50Pa) under the condition of negative pressure to prepare modified polyester, namely low-melting-point polyester; wherein the molar ratio of the terephthalic acid to the ethylene glycol to the 3-chloro-1, 2-butanediol to the diethylene glycol is 1:1.2:0.35:0.12, the addition amount of the catalyst is 0.020% of the mass of the terephthalic acid, and the addition amount of the stabilizer is 0.03% of the mass of the terephthalic acid; the temperature of the esterification reaction was 260 ℃, the end point of the esterification reaction was that the distilled amount of water reached 98% of the theoretical value, the temperature of the polycondensation reaction was 275 ℃, and the reaction time was 50 minutes (wherein the reaction time in the low vacuum stage was 45 minutes);
the number average molecular weight of the prepared low-melting-point polyester is 24300g/mol, the molecular weight distribution D is 2.5, the glass transition temperature is 72 ℃, the melting point is 130 ℃, and the viscous flow activation energy is 30.3 kJ/mol;
(3) preparing low-melting-viscosity low-melting-point polyester fibers;
metering the conventional polyester prepared in the step (1) and the low-melting-point polyester prepared in the step (2) by a metering pump, and then spinning, cooling, bundling, stretching, curling, cutting, drying and packaging according to a skin-core composite spinning process to obtain low-melting-point polyester fibers; wherein the technological parameters are as follows: the spinning temperature is 275 ℃, and the spinning speed is 1200 m/min; the air temperature of the circular blowing air is 23 ℃, and the air speed of the circular blowing air is 8.0 m/s; the drawing multiple is 3.3 times, and the temperature of a drawing oil bath groove is 80 ℃; the drying temperature was 75 ℃.
The finally prepared low-melt-viscosity low-melting-point polyester fiber has a sheath-core structure, the sheath-core ratio is 55:45, the sheath layer is made of low-melting-point polyester, and the core layer is made of conventional polyester; the low melt viscosity and low melting point polyester fiber has a filament fineness of 5dtex, a breaking strength of 4.2cN/dtex, an elongation at break of 55%, a crimp number of 9/25 mm, and a fiber length of 51 mm.
Example 7
A preparation method of low-melting-point fiber flocculus is characterized in that the low-melting-viscosity low-melting-point polyester fiber prepared in example 1, PET (with the length of 51mm and the fineness of 3.3dtex) and three-dimensional curled hollow polyester (with the length of 51mm and the fineness of 6.6dtex) are mixed according to the mass ratio of 15:60:25, and the mixture is carded into a net, thermally dried and shaped to prepare the low-melting-point fiber flocculus with the surface density of 200g/m2The low-melting-point fiber flocculus; wherein the technological parameters are as follows: the hot drying temperature is 145 ℃, the time is 90 seconds, the setting temperature is 170 ℃, and the time is 30 seconds.
The compression elastic rate of the prepared low-melting-point fiber flocculus is 94.2%, the warp breaking strength is 12.88N, and the weft breaking strength is 8.22N; the strength reduction of the low melt fiber batt in the warp and fill directions before and after washing was 11.5% and 14.2%, respectively, as measured by FZ/T64003-1993.
Example 8
A process for preparing low-melting-point fibrous flakes from the low-melting-point fibrous flakes obtained in example 2Mixing the melt viscosity low melting point polyester fiber, PET fiber (length is 51mm, fineness is 3.3dtex) and three-dimensional crimp hollow terylene (length is 51mm, fineness is 6.6dtex) according to the mass ratio of 15:60:25, carding to form a net, hot drying and shaping to obtain the polyester fiber with the surface density of 200g/m2The low-melting-point fiber flocculus; wherein the technological parameters are as follows: the hot drying temperature is 145 ℃, the time is 90 seconds, the setting temperature is 170 ℃, and the time is 30 seconds.
The compression elastic rate of the prepared low-melting-point fiber flocculus is 93.7%, the warp breaking strength is 12.72N, and the weft breaking strength is 8.17N; the strength reduction of the low melt fiber batt in the warp and fill directions before and after washing was 10.3% and 13.1%, respectively, as measured by FZ/T64003-1993.
Example 9
A preparation method of low-melting-point fiber flocculus is characterized in that the low-melting-viscosity low-melting-point polyester fiber prepared in example 3, PET (with the length of 51mm and the fineness of 3.3dtex) and three-dimensional curled hollow polyester (with the length of 51mm and the fineness of 6.6dtex) are mixed according to the mass ratio of 15:60:25, and the mixture is carded into a net, thermally dried and shaped to prepare the low-melting-point fiber flocculus with the surface density of 200g/m2The low-melting-point fiber flocculus; wherein the technological parameters are as follows: the hot drying temperature is 145 ℃, the time is 90 seconds, the setting temperature is 170 ℃, and the time is 30 seconds.
The compression elastic rate of the prepared low-melting-point fiber flocculus is 95.1%, the warp breaking strength is 13.11N, and the weft breaking strength is 8.32N; the strength reduction of the low melt fiber batt in the warp and fill directions before and after washing was 12.9% and 15.7%, respectively, as measured by FZ/T64003-1993.
Example 10
A preparation method of low-melting-point fiber flocculus is characterized in that the low-melting-viscosity low-melting-point polyester fiber prepared in example 4, PET (with the length of 51mm and the fineness of 3.3dtex) and three-dimensional curled hollow polyester (with the length of 51mm and the fineness of 6.6dtex) are mixed according to the mass ratio of 15:60:25, and the mixture is carded into a net, thermally dried and shaped to prepare the low-melting-point fiber flocculus with the surface density of 200g/m2The low-melting-point fiber flocculus; wherein the technological parameters are as follows: the hot drying temperature is 145 ℃, the time is 90 seconds, and the setting temperature is170 ℃ for 30 seconds.
The compression elastic rate of the prepared low-melting-point fiber flocculus is 94.2%, the warp breaking strength is 13.21N, and the weft breaking strength is 8.17N; the strength reduction of the low melt fiber batt in the warp and fill directions before and after washing was 11.2% and 15.3%, respectively, as measured by FZ/T64003-1993.
Example 11
A preparation method of low-melting-point fiber flocculus is characterized in that the low-melting-viscosity low-melting-point polyester fiber prepared in example 5, PET (with the length of 51mm and the fineness of 3.3dtex) and three-dimensional curled hollow polyester (with the length of 51mm and the fineness of 6.6dtex) are mixed according to the mass ratio of 15:60:25, and the mixture is carded into a net, thermally dried and shaped to prepare the low-melting-point fiber flocculus with the surface density of 200g/m2The low-melting-point fiber flocculus; wherein the technological parameters are as follows: the hot drying temperature is 145 ℃, the time is 90 seconds, the setting temperature is 170 ℃, and the time is 30 seconds.
The compression elastic rate of the prepared low-melting-point fiber flocculus is 93.6%, the warp breaking strength is 12.84N, and the weft breaking strength is 8.31N; the strength reduction of the low melt fiber batt in the warp and fill directions before and after washing was 12.0% and 14.4%, respectively, as measured by FZ/T64003-1993.
Example 12
A preparation method of low-melting-point fiber flocculus is characterized in that the low-melting-viscosity low-melting-point polyester fiber prepared in example 6, PET (polyethylene terephthalate) fiber (the length is 51mm, and the fineness is 3.3dtex) and three-dimensional curled hollow polyester (the length is 51mm, and the fineness is 6.6dtex) are mixed according to the mass ratio of 15:60:25, and the mixture is carded into a net, thermally dried and shaped to prepare the low-melting-point fiber flocculus with the surface density of 200g/m2The low-melting-point fiber flocculus; wherein the technological parameters are as follows: the hot drying temperature is 145 ℃, the time is 90 seconds, the setting temperature is 170 ℃, and the time is 30 seconds.
The compression elastic rate of the prepared low-melting-point fiber flocculus is 94.8%, the warp breaking strength is 13.07N, and the weft breaking strength is 8.36N; the strength reduction of the low melt fiber batt in the warp and fill directions before and after washing was 11.5% and 13.6%, respectively, as measured by FZ/T64003-1993.

Claims (10)

1. A low melt viscosity low melt polyester fiber characterized by: the low-melt-viscosity low-melting-point polyester fiber has a sheath-core structure, the sheath layer is made of low-melting-point polyester, and the core layer is made of conventional polyester;
the low-melting-point polyester is modified polyester, and a molecular chain of the modified polyester consists of a terephthalic acid chain segment, an ethylene glycol chain segment, a 3-chloro-1, 2-butanediol chain segment and a diethylene glycol chain segment; the molecular chain of the conventional polyester consists of a terephthalic acid chain segment and an ethylene glycol chain segment;
the low-melting-point polyester has a glass transition temperature of 68-72 ℃, a melting point of 100-130 ℃ and a viscous flow activation energy of 21.6-30.3 kJ/mol.
2. The polyester fiber with low melting viscosity and low melting point as claimed in claim 1, wherein the molecular chain of the modified polyester has a molar ratio of a terephthalic acid segment, an ethylene glycol segment, a 3-chloro-1, 2-butanediol segment and a diethylene glycol segment of 1: 0.53-0.62: 0.29-0.34: 0.09-0.13; the molar ratio of the terephthalic acid chain segment to the ethylene glycol chain segment in the molecular chain of the conventional polyester is 1:1.
3. The polyester fiber with low melting viscosity and low melting point as claimed in claim 1, wherein the polyester fiber with low melting viscosity and low melting point has a filament fineness of 4 to 5dtex, a breaking strength of not less than 3.8cN/dtex, an elongation at break of 50 to 60%, a number of crimps of 8 to 12/25 mm, and a fiber length of 51 mm.
4. The polyester fiber with low melting viscosity and low melting point as claimed in claim 1, wherein the sheath-core ratio of the sheath-core structure is 45-55: 55-45.
5. The low melt viscosity and low melting point polyester fiber according to claim 1, wherein the number average molecular weight of the low melting point polyester is 20000 to 25000g/mol, and the molecular weight distribution D is 2.2 to 3.0.
6. The method for preparing the low-melt-viscosity low-melting-point polyester fiber according to any one of claims 1 to 5, comprising the steps of:
(1) preparing conventional polyester;
preparing terephthalic acid, ethylene glycol, a catalyst and a stabilizer into slurry, carrying out esterification reaction, and after the esterification reaction is finished, sequentially carrying out polycondensation reaction in a low vacuum stage and polycondensation reaction in a high vacuum stage under the condition of negative pressure to prepare conventional polyester; the pressure of the polycondensation reaction in the low vacuum stage is 5000-500 Pa, and the pressure of the polycondensation reaction in the high vacuum stage is less than 100 Pa;
(2) preparing low-melting-point polyester;
preparing terephthalic acid, ethylene glycol, 3-chloro-1, 2-butanediol, diethylene glycol, a catalyst and a stabilizer into slurry, and then carrying out esterification reaction to obtain an esterification product; after the esterification reaction is finished, heating, stirring and mixing, and sequentially carrying out the polycondensation reaction in a low vacuum stage and the polycondensation reaction in a high vacuum stage under the condition of negative pressure to prepare modified polyester, namely low-melting-point polyester; the pressure of the polycondensation reaction in the low vacuum stage is 5000-500 Pa, and the pressure of the polycondensation reaction in the high vacuum stage is less than 100 Pa;
(3) preparing low-melting-viscosity low-melting-point polyester fibers;
and (2) metering the conventional polyester prepared in the step (1) and the low-melting-point polyester prepared in the step (2) by a metering pump, and then spinning, cooling, bundling, stretching, curling, cutting, drying and packaging according to a skin-core composite spinning process to obtain the low-melting-point polyester fiber.
7. The process according to claim 6, wherein the temperature of the esterification reaction in the step (1) is 240 to 260 ℃, the end point of the esterification reaction is that the distilled amount of water reaches 95% or more of the theoretical value, the temperature of the polycondensation reaction is 275 to 280 ℃, and the reaction time is 60 to 90 minutes;
in the step (2), the temperature of the esterification reaction is 220-260 ℃, the end point of the esterification reaction is that the distilled amount of water reaches more than 95% of a theoretical value, the temperature of the polycondensation reaction is 265-275 ℃, and the reaction time is 50-90 minutes;
the technological parameters in the step (3) are as follows: the spinning temperature is 270-275 ℃, and the spinning speed is 1000-1200 m/min; the air temperature of the circular blowing air is 20-23 ℃, and the air speed of the circular blowing air is 7.0-8.0 m/s; the drawing multiple is 2.5-3.3 times, and the temperature of a drawing oil bath groove is 75-80 ℃; the drying temperature is 70-75 ℃.
8. The method according to claim 6, wherein the molar ratio of terephthalic acid to ethylene glycol in step (1) is 1:1.3 to 1.6;
in the step (2), the molar ratio of the terephthalic acid to the ethylene glycol to the 3-chloro-1, 2-butanediol to the diethylene glycol is 1: 1.1-1.3: 0.30-0.35: 0.08-0.12;
the catalyst in the step (1) and the step (2) is antimony trioxide, ethylene glycol antimony or antimony acetate, the stabilizer is triphenyl phosphate, trimethyl phosphate or trimethyl phosphite, the adding amount of the catalyst is 0.018 to 0.020 percent of the mass of the terephthalic acid, and the adding amount of the stabilizer is 0.01 to 0.03 percent of the mass of the terephthalic acid.
9. The use of the low melt viscosity low melt polyester fiber according to any one of claims 1 to 5, wherein: mixing low-melting-viscosity low-melting-point polyester fibers with other fibers according to a certain proportion, and then carding, forming a web, baking and shaping to prepare low-melting-point fiber flocculus;
the other fibers refer to PET fibers and three-dimensional curled hollow polyester;
the surface density of the low-melting-point fiber flocculus is 200g/m2(ii) a The low-melting-point fiber flocculus has the compression elasticity rate of 93.7-95.1%, the warp-wise breaking strength of 12.72-13.21N and the weft-wise breaking strength of 8.17-8.36N; the strength reduction rate of the low-melting-point fiber flocculus in the warp direction and the weft direction is 10.3-12.9% and 13.1-15.7% respectively before and after washing according to the FZ/T64003-1993 test.
10. Use according to claim 9, characterized in that: the mass ratio of the low-melting-viscosity low-melting-point polyester fibers to the PET fibers to the three-dimensional curled hollow polyester fibers is 15:60: 25;
the length of the PET fiber is 51mm, and the fineness is 3.3 dtex; the length of the three-dimensional curled hollow polyester is 51mm, and the fineness is 6.6 dtex.
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